Hydrazine hydrate (1:1) → 1-[3-(Amino)propan-1-yl]-1,2-dihydro-3-methyl-1,4,7b-triazacyclopent[cd]inden-2-one

HRID 619513노트

반응식

HRID 619513 반응식
[CH3:1][C:2]1[N:3]=[C:4]2[CH:12]=[CH:11][CH:10]=[C:9]3[N:5]2[C:6]=1[C:7](=[O:27])[N:8]3[CH2:13][CH2:14][CH2:15][N:16]1C(=O)C2=CC=CC=C2C1=O.O.NN>C(O)C>[NH2:16][CH2:15][CH2:14][CH2:13][N:8]1[C:9]2[N:5]3[C:4](=[N:3][C:2]([CH3:1])=[C:6]3[C:7]1=[O:27])[CH:12]=[CH:11][CH:10]=2

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 21190099HCID 21190099, 화합물

생성물 1

HCID 211900961-[3-(Amino)propan-1-yl]-1,2-dihydro-3-methyl-1,4,7b-triazacyclopent[cd]inden-2-one수율 75.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a suspension of 3.47 g (9.63 mmol) of 1,2-dihydro-3-methyl-1-[3-(phthalimido)propan-1-yl]-1,4,7b-triazacyclopent[cd]inden-2-one in 70 ml of ethanol was added 1.45 g (29.0 mmol) of hydrazine monohydrate. The mixture was heated for 2 hours under reflux. After cooling, and the resulting precipitates were filtered off. The filtrate was concentrated to give the residue, water was added, extracted with chloroform (three times). The extract was dried over anhydrous magnesium sulfate, then the solvent was distilled off to give 1.68 g of the desired compound (75.8%, pale yellow solid substance).

후처리

  1. temperatureThe mixture was heated for 2 hours
  2. temperatureunder reflux
  3. temperatureAfter cooling
  4. customthe resulting precipitates
  5. filtrationwere filtered off
  6. concentrationThe filtrate was concentrated
  7. customto give the residue, water
  8. additionwas added
  9. extractionextracted with chloroform (three times)
  10. dry with materialThe extract was dried over anhydrous magnesium sulfate
  11. distillationthe solvent was distilled off

출처 및 근거

ORD 기록
ord-aa66cb799c7341ea84c01ace696e288a
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05958942

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